CN111139526A - Method for obtaining single crystal boron nitride film by ion beam sputtering deposition - Google Patents
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- CN111139526A CN111139526A CN202010063893.XA CN202010063893A CN111139526A CN 111139526 A CN111139526 A CN 111139526A CN 202010063893 A CN202010063893 A CN 202010063893A CN 111139526 A CN111139526 A CN 111139526A
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
The invention relates to the research field of two-dimensional layered materials, in particular to a method for obtaining a single-crystal boron nitride film by utilizing ion beam sputtering deposition. The method comprises the following steps: ultrasonically cleaning a single crystal substrate by using acetone, ethanol and deionized water in sequence; immersing the cleaned single crystal substrate into a hydrofluoric acid solution for treatment; arranging a high-purity Ni target on a target position of a direct-current magnetron sputtering instrument, and epitaxially growing a Ni (111) -oriented film on a single crystal substrate; fixing a nickel/single crystal substrate on a sample holder, placing the sample holder into a growth chamber of ion beam sputtering deposition equipment, and performing film growth through hydrogen and argon treatment; and cooling the grown film to obtain the large-size single crystal boron nitride film.
Description
Technical Field
The invention relates to the research field of two-dimensional layered materials, which is mainly applied to the fields of insulation, heat conduction, deep ultraviolet luminescence, gate dielectric layers, microwave shielding and the like, and particularly relates to a method for obtaining a single crystal boron nitride film by utilizing ion beam sputtering deposition.
Background
The hexagonal boron nitride (h-BN) film is taken as an important material in the field of two-dimensional materials, and is expected to be widely applied to the fields of insulating substrates, deep ultraviolet luminescence, dielectric materials, microwave shielding and the like due to the characteristics of extremely high in-plane elastic modulus, atomically smooth surface, wide forbidden band (5.9eV), good insulativity, high-temperature stability, chemical stability, high thermal conductivity and the like. The h-BN two-dimensional atomic crystal is prepared by a Chemical Vapor Deposition (CVD) technology, but the H-BN two-dimensional atomic crystal has the defects of a large number of precursors, complex and unclear growth mechanism, a large number of defects in a product, serious influence on the performance of a film, high price of the used organic precursors, most of the used organic precursors are highly toxic substances, the defects of a large number of byproducts, poor stability and the like, and the H-BN two-dimensional atomic crystal is not favorable for realizing large-scale production. The invention improves the defects of complex growth process, unstable precursor and poor controllability of the h-BN film.
Disclosure of Invention
The invention relates to a method for obtaining a single crystal boron nitride film by ion beam sputtering deposition, which can obtain a large-size single crystal boron nitride film with high quality and low cost, the size of the single crystal boron nitride film can be obviously improved,
the specific scheme is as follows:
a method for obtaining a single crystal boron nitride film by ion beam sputter deposition, comprising:
s1, ultrasonically cleaning a single crystal substrate by using acetone, ethanol and deionized water in sequence;
s2, immersing the cleaned single crystal substrate into a hydrofluoric acid solution for treatment;
s3, arranging a high-purity Ni target on a target position of a direct-current magnetron sputtering instrument, and epitaxially growing a Ni (111) -oriented film on a single crystal substrate;
s4, fixing the nickel/single crystal substrate on a sample support, placing the sample support into a growth chamber of ion beam sputtering deposition equipment, processing the film in a hydrogen atmosphere, and growing the film in an argon atmosphere;
and S5, cooling the grown film to obtain the large-size single crystal boron nitride film.
In the step S1, when the ultrasonic cleaning is performed in sequence by using acetone, ethanol and deionized water, the ultrasonic cleaning is performed by using the deionized water after each cleaning, and finally the ultrasonic cleaning is performed by drying.
And (3) after the single crystal substrate in the S2 is immersed in the hydrofluoric acid solution for 20-30S, washing the single crystal substrate with deionized water, and finally drying the single crystal substrate.
In the S3, the purity of the high-purity Ni target is 99.99%.
The S4 further includes:
s401, fixing a nickel/single crystal substrate on a sample support, placing the sample support into a growth chamber of ion beam sputtering deposition equipment, and vacuumizing the chamber to 3.75 multiplied by 10-3mTor；
S402, introducing hydrogen into the reaction chamber, and annealing the nickel/single crystal substrate after heating;
s403, closing a hydrogen valve, introducing argon, and after the air pressure is stable, opening a furnace plate to rotate and a main ion source to generate Ar ions;
s404, setting sputtering bias voltage, accelerating voltage and anode voltage, adjusting cathode filament current, and growing the film.
In S5, the grown film was naturally cooled to room temperature under argon.
The invention has the beneficial effects that: the preparation of the h-BN film is simple and controllable, and the growth of the film can be effectively controlled by adjusting the deposition conditions; the preparation process effectively overcomes the defects of high cost and high toxicity of the prior art and is more environment-friendly; the prepared film has larger size and controllable layer number, and can realize the preparation of large-area h-BN films.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a large-sized h-BN single crystal film;
FIG. 2 is an SEM image of h-BN single-crystal domains grown on the surface of a Ni epitaxial thin film;
FIG. 3 is a Raman spectrum of the h-BN single crystal thin film in example 1;
FIG. 4 is a Raman spectrum of the h-BN single crystal thin film in example 2;
FIG. 5 is a Raman spectrum of the h-BN single crystal thin film in example 3;
FIG. 6 is a Raman spectrum of the h-BN single crystal thin film in example 4;
FIG. 7 is a Raman spectrum of the h-BN single crystal thin film in example 5.
Detailed Description
The invention is explained in more detail below with reference to the figures and the examples, without limiting the scope of protection of the invention to these examples. In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Example 1:
a. ultrasonically cleaning a c-surface sapphire substrate for 10min by using acetone, ethanol and deionized water in sequence, washing with the deionized water after each cleaning is finished, and finally drying in a constant temperature box;
b. immersing the cleaned sapphire substrate into a hydrofluoric acid solution (with the mass fraction of 10%) for 30s, washing with deionized water, and drying the substrate in a vacuum drying oven;
c. placing a high-purity Ni target (purity 99.99%) on a target position of a direct current magnetron sputtering apparatus, and epitaxially growing a Ni (111) -oriented thin film with a thickness of 2.5 μm on a sapphire substrate heated to 600 ℃ in an argon atmosphere at a constant power of 50W;
d. fixing the sputtered Ni/sapphire substrate on a sample support, placing the sample support into a growth chamber, vacuumizing the chamber to 3.75 multiplied by 10 < -3 > mTor, introducing 50sccm hydrogen into the reaction chamber to increase the air pressure to 30mTor, and increasing the heating current to increase the temperature of the substrate to 1030 ℃ for annealing for 10 min;
e. after annealing, closing a hydrogen valve, introducing argon of 4sccm, and after the air pressure is stabilized to 30mTor, opening a furnace disc to rotate and a main ion source (generating Ar ions);
f. setting sputtering bias voltage to 1000V, accelerating voltage to 200V and anode voltage to 120V, adjusting cathode filament current to enable beam current to be 18mA, and growing for 30 min;
g. and naturally cooling the grown film to room temperature in argon to obtain the large-size single crystal boron nitride film.
Example 2:
a. ultrasonically cleaning a c-surface sapphire substrate for 10min by using acetone, ethanol and deionized water in sequence, washing with the deionized water after each cleaning is finished, and finally drying in a constant temperature box;
b. immersing the cleaned sapphire substrate into a hydrofluoric acid solution (with the mass fraction of 10%) for 30s, washing with deionized water, and drying the substrate in a vacuum drying oven;
c. placing a high-purity Ni target (purity is 99.99%) on a target position of a direct-current magnetron sputtering instrument, and carrying out epitaxial growth on a Ni (111) -oriented thin film with the thickness of 2.5 microns on a sapphire substrate which is heated to 600 ℃ in an argon atmosphere at a constant power of 60W;
d. fixing the sputtered Ni/sapphire substrate on a sample support, placing the sample support into a growth chamber, vacuumizing the chamber to 3.75 multiplied by 10 < -3 > mTor, introducing 50sccm hydrogen into the reaction chamber to increase the pressure of the gas to 40mTor, and increasing the heating current to increase the temperature of the substrate to 1050 ℃ for annealing for 10 min;
e. after annealing, a hydrogen valve is closed, argon gas of 4sccm is introduced, and after the gas pressure is stabilized to 40mTor, the furnace plate is turned on to rotate and the main ion source is started (Ar ions are generated).
f. Setting sputtering bias voltage to 1000V, accelerating voltage to 200V and anode voltage to 120V, adjusting cathode filament current to enable beam current to be 15mA, and growing for 30 min;
g. and naturally cooling the grown film to room temperature in argon to obtain the large-size single crystal boron nitride film.
Example 3:
a. ultrasonically cleaning a c-surface sapphire substrate for 10min by using acetone, ethanol and deionized water in sequence, washing with the deionized water after each cleaning is finished, and finally drying in a constant temperature box;
b. immersing the cleaned c-surface sapphire substrate into a hydrofluoric acid solution (the mass fraction is 10%) for 30s, washing the substrate with deionized water, and drying the substrate in a vacuum drying oven;
c. placing a high-purity Ni target (purity 99.99%) on a target position of a direct current magnetron sputtering instrument, and epitaxially growing a Ni (111) -oriented thin film with a thickness of 2.5 μm on a sapphire substrate heated to 600 ℃ in an argon atmosphere at a constant power of 70W;
d. fixing the sputtered Ni/sapphire substrate on a sample support, placing the sample support into a growth chamber, vacuumizing the chamber to 3.75 multiplied by 10 < -3 > mTor, introducing 50sccm hydrogen into the reaction chamber to increase the air pressure to 50mTor, and increasing the heating current to increase the temperature of the substrate to 1070 ℃ for annealing for 10 min;
e. after annealing, a hydrogen valve is closed, argon gas of 4sccm is introduced, and after the gas pressure is stabilized to 50mTor, the furnace plate is opened to rotate and the main ion source is started (Ar ions are generated).
f. Setting sputtering bias voltage to 1000V, accelerating voltage to 200V and anode voltage to 120V, adjusting cathode filament current to make beam current 12mA, and growing for 30 min;
g. and naturally cooling the grown film to room temperature in argon to obtain the large-size single crystal boron nitride film.
Example 4:
a. ultrasonically cleaning the MgO single crystal substrate for 10min by using acetone, ethanol and deionized water in sequence, washing with the deionized water after each cleaning is finished, and finally drying in a constant temperature box;
b. immersing the cleaned MgO single crystal substrate into a hydrofluoric acid solution (the mass fraction is 10%) for 30s, washing the substrate with deionized water, and drying the substrate in a vacuum drying oven;
c. placing a high-purity Ni target (purity 99.99%) on a target position of a direct current magnetron sputtering apparatus, and epitaxially growing a 2.5 μm-thick Ni (111) -oriented thin film on an MgO substrate heated to 600 ℃ in an argon atmosphere at a constant power of 55W;
d. fixing the sputtered Ni/MgO substrate on a sample support, placing the sample support into a growth chamber, vacuumizing the chamber to 3.75 multiplied by 10 < -3 > mTor, introducing 50sccm hydrogen into the reaction chamber to increase the air pressure to 60mTor, and increasing the heating current to increase the temperature of the substrate to 1030 ℃ for annealing for 10 min;
e. and after annealing, closing a hydrogen valve, introducing argon of 4sccm, and after the air pressure is stabilized to 60mTor, opening the furnace disc to rotate and a main ion source (generating Ar ions).
f. Setting sputtering bias voltage to 1000V, accelerating voltage to 200V and anode voltage to 120V, adjusting cathode filament current to enable beam current to be 18mA, and growing for 30 min;
g. and naturally cooling the grown film to room temperature in argon to obtain the large-size single crystal boron nitride film.
Example 5:
a. ultrasonically cleaning the MgO single crystal substrate for 10min by using acetone, ethanol and deionized water in sequence, washing with the deionized water after each cleaning is finished, and finally drying in a constant temperature box;
b. immersing the cleaned MgO single crystal substrate into a hydrofluoric acid solution (the mass fraction is 10%) for 30s, washing the substrate with deionized water, and drying the substrate in a vacuum drying oven;
c. placing a high-purity Ni target (purity 99.99%) on a target position of a direct current magnetron sputtering apparatus, and epitaxially growing a 2.5 μm-thick Ni (111) -oriented thin film on an MgO substrate heated to 600 ℃ at a constant power of 65W in an argon atmosphere;
d. fixing the sputtered Ni/MgO substrate on a sample support, placing the sample support into a growth chamber, vacuumizing the chamber to 3.75 multiplied by 10 < -3 > mTor, introducing 50sccm hydrogen into the reaction chamber to increase the air pressure to 70mTor, and increasing the heating current to increase the temperature of the substrate to 1050 ℃ for annealing for 10 min;
e. and after annealing, closing a hydrogen valve, introducing argon of 4sccm, and after the air pressure is stabilized to 70mTor, opening the furnace disc to rotate and a main ion source (generating Ar ions).
f. Setting sputtering bias voltage to 1000V, accelerating voltage to 200V and anode voltage to 120V, adjusting cathode filament current to enable beam current to be 15mA, and growing for 30 min;
g. and naturally cooling the grown film to room temperature in argon to obtain the large-size single crystal boron nitride film.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. A method for obtaining a single crystal boron nitride film by ion beam sputter deposition, comprising:
s1, ultrasonically cleaning a single crystal substrate by using acetone, ethanol and deionized water in sequence;
s2, immersing the cleaned single crystal substrate into a hydrofluoric acid solution for treatment;
s3, arranging a high-purity Ni target on a target position of a direct-current magnetron sputtering instrument, and epitaxially growing a Ni (111) -oriented film on a single crystal substrate;
s4, fixing the nickel/single crystal substrate on a sample support, placing the sample support into a growth chamber of ion beam sputtering deposition equipment, processing the film in a hydrogen atmosphere, and growing the film in an argon atmosphere;
and S5, cooling the grown film to obtain the large-size single crystal boron nitride film.
2. The method of claim 1 for obtaining a single crystal boron nitride film by ion beam sputter deposition, wherein: in the step S1, when the ultrasonic cleaning is performed in sequence by using acetone, ethanol and deionized water, the ultrasonic cleaning is performed by using the deionized water after each cleaning, and finally the ultrasonic cleaning is performed by drying.
3. The method of claim 1 for obtaining a single crystal boron nitride film by ion beam sputter deposition, wherein: and (3) after the single crystal substrate in the S2 is immersed in the hydrofluoric acid solution for 20-30S, washing with deionized water, and finally drying the single crystal substrate.
4. The method of claim 1 for obtaining a single crystal boron nitride film by ion beam sputter deposition, wherein: in the S3, the purity of the high-purity Ni target is 99.99%.
5. The method of claim 1 for obtaining a single crystal boron nitride film by ion beam sputter deposition, wherein: the S4 further includes:
s401, fixing a nickel/single crystal substrate on a sample support, placing the sample support into a growth chamber of ion beam sputtering deposition equipment, and vacuumizing the chamber to 3.75 multiplied by 10 < -3 > mTor;
s402, introducing hydrogen into the reaction chamber, and annealing the nickel/single crystal substrate after heating;
s403, closing a hydrogen valve, introducing argon, and after the air pressure is stable, opening a furnace plate to rotate and a main ion source to generate Ar ions;
s404, setting sputtering bias voltage, accelerating voltage and anode voltage, adjusting cathode filament current, and growing the film.
6. The method of claim 1 for obtaining a single crystal boron nitride film by ion beam sputter deposition, wherein: in S5, the grown film was naturally cooled to room temperature under argon.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621845A (en) * | 2020-05-26 | 2020-09-04 | 中国人民解放军国防科技大学 | Preparation method of inch-grade single crystal film and single crystal film |
| CN115261978A (en) * | 2022-08-29 | 2022-11-01 | 东南大学 | Method for preparing multilayer boron nitride film with ferroelectric AB stack |
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| CN101323982A (en) * | 2008-07-16 | 2008-12-17 | 上海大学 | Preparation of high quality cubic boron nitride film |
| CN104313684A (en) * | 2014-09-30 | 2015-01-28 | 中国科学院半导体研究所 | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal |
| CN108193276A (en) * | 2017-12-28 | 2018-06-22 | 中国科学院半导体研究所 | The method for preparing the single-orientated hexagonal boron nitride two-dimensional atomic crystal of large area |
| CN110629184A (en) * | 2019-10-18 | 2019-12-31 | 中国科学院半导体研究所 | Method for directly growing two-dimensional hexagonal boron nitride on dielectric substrate |
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2020
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| CN101323982A (en) * | 2008-07-16 | 2008-12-17 | 上海大学 | Preparation of high quality cubic boron nitride film |
| CN104313684A (en) * | 2014-09-30 | 2015-01-28 | 中国科学院半导体研究所 | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal |
| CN108193276A (en) * | 2017-12-28 | 2018-06-22 | 中国科学院半导体研究所 | The method for preparing the single-orientated hexagonal boron nitride two-dimensional atomic crystal of large area |
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| JUNHUA MENG,ET AL.: "Aligned Growth of Millimeter-Size Hexagonal Boron Nitride Single-Crystal Domains on Epitaxial Nickel Thin Film", 《ADVANCED SCIENCE NEWS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621845A (en) * | 2020-05-26 | 2020-09-04 | 中国人民解放军国防科技大学 | Preparation method of inch-grade single crystal film and single crystal film |
| CN115261978A (en) * | 2022-08-29 | 2022-11-01 | 东南大学 | Method for preparing multilayer boron nitride film with ferroelectric AB stack |
| CN115261978B (en) * | 2022-08-29 | 2023-08-04 | 东南大学 | Method for preparing AB-stacked multilayer boron nitride film with ferroelectricity |
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Application publication date: 20200512 |